Apparatus for dividing air into its elements by fractional distillation.



' M. HAZA RD-FLAMAND.

' APPARATUS FDA: DIVIDING AI R INTO ITS ELEMENTS BY FRACTIONAL DISTILLATION.

' APPLICATION FILED DEC.9, 190 8.

Patented 0%- 10, 1916.

3 SHEETS-SHEET l.

APPARATUS FOR DIV|D| NG AIR INTO ITS ELEMENTS BY FRACTIONAL DISTILLATION. v

. APPUCATION FILED DEC. 9, I908- 1,201,043. Patented Oct. 10,1916.

.3SHETS-SH E ET 3.

E I I a wdvwwey jnu'enbot man-monnAzAnn-rmmmn, on ST. vnam, Eamon.-

Q nrrm'rusron nrvrome Ant INTO .ITS'ELEHENTS BY rnAc'rronAL DISTILLATION.

To (ill whom it may concern;

Be it known that I, MAURICE HAZARD FLAMAND, whose post oflicepaddress is St.

Vrain, Seine-et-Oise,-France, have invented I 5 certain 'new and useful Improvements in Apparatus for Dividing Air into Its Elements by Fractional Distillation, ofwhich the following is aspecification.

-My invention-relates to an apparatus for producing oxygen and nitrogen and more particularly to the-production of these gases y means of an apparatus wherein the air is separated into its constituents by being subjected to low temperature conditions.

By my invention, I am enabled to produce oxygen and nitrogen from air by ,a frac- 'tional distillation process, the practice of which does not require the air to be liquefied before treatment. By this method,'I- separate the nitrogen and the oxygen under con' ditions which will insure substantially pure gases, a'pp'roximating in volume the percentage of each gas contained inthe air subjected tothe treatment. My improved art or methodutilizes nitrogen, ata pressure and a temperature {which will liquefy 0xy-. gen, asthe mea nsfor 'efi'ecting-the separa-' tion of the constituents of the air and hence a portion of the 'products secured by the practice of my method, may be "utilized in l a continuance ofthe practice and not only.

admit of a continuous method of separating the gases of the air, ,but an economical method as well. My improved method requiresthe maintenance of low-temperatures during allsteps thereof, and in the practice 7 of the invention, I arrange toabstract from the air to be subjected to the treatment as high a percentage of the heat units as is 4:0 practicable for the successful practice of my method, utilizing the gases being produced for this purpose. Ialso utilize the relatively higher temperature of the gaseous oxygen produced by my inethod, for conditioning -the nitrogen fused in converting the liquid oxygen to gaseous form and the nitrogen used-inlowering the temperature of the air .to the temperature of its saturated vapors. Furthermore, -I utilize the liqu d oxygen in liquefyin or otherwise conditioning the nitrogen to be used in the distilling column in chamber with the incidental vaporization Trend oxygen.

The method above referred. to is not i I s peeification of Letters Patent. i Patented Oct, 10, 1916, APP l tation filed December 9, 1908 Serial No. 466,683. i

. claimedh'erein, the same being made the sub ect matter 'of a divisional application. In the apparatus for carrying on my aforesaid method or art, I provide in con- 1 1nct1on with one or more multiple stage distilling columns, means whereby the atmospheric air before being delivered to said distilling column or colunms is brought to the temperature of. its saturated vapors and means for maintaining a continuous circulation of nitrogen] startin from the nitrogen delivery end of the distilling column or 001- umnsin-thehform of a gas and ending adjacent said outlet in the form of a liquid, suitable devices being arranged intermediate said points for utilizing the heat units of said nitrogen in carrying on the aforesaid method. I also provide in conjunction with said distilling column or columns means for separating the liquid oxygen and subjecting the separated bodies'to the action of the nitrogen in a manner to gasify said oxygen I for the two-fold object of utilizing a portion of said gases iii the distilling column and conditioning another portion thereof for withdrawal from the apparatus. as a product. I 'also provide means 1 whereby the products of the machine are utilized in maintaining the low temperatures throughout the apparatus necessary to the successful operation thereof. I In conditioning the air, I preferably employ a device in which the nitrogen'used in the distilling-operation aids in developing the necessary low temperatures in the air under treatment and in which impurities in the air will be removed prior to its introduction to the distilling column so a s -to permit the I production of substantially pure oxygen and substantially pure nitrogen.

The invention consists in an apparatus for I dividing air into its elements embodying the 1 novel features of construction and combination of parts all as hereinafter set forth and *describedand more in the, claims hereto appended. Referring to the drawings:

view partly in elevation and partly in section of "an apparatus embodying my invention}; Fig. 2 shows a modification thereof by whichithe desired low temperatures may be maintained throughout-'- the distilling ,col-

' 't ion' for the same purpose; Figs. 1,5-and 6 Figure l is. a

- .umn; Fig. 3is a'viewof a further modificaa be precipitated and will 80 municates.

show modifications in the construction of the apparatus shown in Fig. 1; and Figs. 7 and 8 show an, apparatus which may be used in conjunction with a distilling column for clarifying the upper portion thereof.

Like letters refer to like parts throughout the several views. a V

In the apparatus shown in Fig. 1 mths accompanying drawings, I employ a multiple stage distilling column 6, discharging into which is a pipe 7 adapted to deliver anat the temperature of its saturated vapors. This pipe communicates with said column at a stage intermediate the top and bottom thereof at a point where the temperature of the column will be substantially that of the vapors introduced thereto. The air at any desired or necessary'pressure is delivered into the apparatus through the pipe 1 which has a nozzle 3 discharging into a refrigerating chamber at with which the pipe 7 com- It is'in this chamber that the air to be treated is brought to the temperature of its saturated'va-pors, suitable means being provided in conjunction with this chamber for bringing the air to the desired temperature. Incidentally in bringing the air to this temperature impurities will accumulate in the bottom of the chamber. The bottom of the column is provided with a boiler 23 adapted to receive the liquefied oxygen and surrounding this boiler is a chamber 26, from which oxygen in the boiler is adapted to flow through the tube 25 thus dividing the liquid oxygen so thatthe portion thereof within the boiler 26 will be in direct communication with the stages of the distilling column while the portion 26 will'be separatated from the distilling column in-a manner to permit the'withdrawal of the gaseous oxygen therefrom as. a product of the apparatus. Below the boiler 23 and vaporizer 26 is' a condensing chamber or balloon 101 adapted to receive the nitrogen being constantly circulated through the apparatus and expose the surface of said boiler and said vaporizer to the action of this nitrogenin a manner to gasify the oxygen contained therein with a resultant condensation of said nitrogen. Leading from said condensing chamber or balloon 101 and discharging into the upper portion of the distilling column 6 is a pipe 32 having a valve 33 arranged inthe length-thereof for controlling the rate of, flow of the nitrogen from said chamber to the upper portion of the "distilling column. As heretofore described, the air upon entering the column 6 is gradually separated by fractional distillation-into its constituents, the oxygen descen'ding from stageto stage and the nitrogen ascending from stage to stage until it,

'in the" upper. portion of the column, is in a V gaseous condition. The gaseous nitrogen is withdrawn from the column through" the nitrogen offtake pipe having in its length the exchanger 2 through which the pipe 1 passes so as to utilize the low temperature of this gas in raising the temperature of the air under treatment. In the length of said pipe isan oiftake opening '27 from which a portion of the nitrogen withdrawn from the distilling column .is removed as a product of the apparatus. The said gases are withdrawn from the column by means of the compressor 28 or any equivalent device which pass these gases through a refrigerator 29 and the pipe 31 to the tubes 5 within the chamber 4 and thence through the pipe containing in its length the valve 18 to the condensing chamber or balloon 101. It will thus be seen that I provide means for condicatcd at 35. By this construction. it will be observed that the heat exchangers 2 and 30 are maintained at a low temperature by the nitrogen withdrawn from the upper portion of the distilling column and from the oxygen withdrawn from the apparatus as a product; that the exchanger 2 acts to lower the temperature of the air introduced in the apparatus and the nitrogen being delivered to the condensing chamber, and that the exchanger 30 serves to raise the temperature of the oxygen being delivered from the apparatus and to lower the temperature of the nitrogen passing to the said condens ing chamber or balloon. By passing the nitrogen through the tubes 5, I utilize this circulating nitrogen for lowering the temperature of the air to be treated while passing through the refrigerating chamber 4. Oxygen may also be withdrawn either in a liquid or gaseous state by means of the valve controlled pipe 36.

Other means than the refrigerating. chamber 4 and its appurtenances may be used for bringing the air to the temperature of its saturated vapors, Fig. 2 and Fig. 3 each illustrating a refrigerating mechanism which may be used in conjunction with the distilling column 6 and its appurtenances for conditioning the air preparatory to its delivery to said column.

In the modification shown in Fig. 2,- inenters through the pipe 8 flows upwardly .13 which receives liquid air through the pipe 12 from the bottom of the chamber 9. The apparatus shownin Fig. 2 may be used as a substitute for the refrigerating cham-- this form,

let of said coil 16*,

other desired source,

ber 4 and its appurtenances.- In Fig. 3. I have shown an apparatus for supplying this cold of compensation utilizing nitrogen. In

the upper portion of the distilling column is provided, with a tank 15 receiving liquid nitrogen through the pipe -14. Arranged in this tank is a coil 16' through which the air to be treated is passed, theoutshown to the right of the figure, delivering the air at the desired stage of the distilling column. The nitrogen delivered through the pipe 14 may come from the condensing chamber or balloon 101 or in part therefrom and in part from any the overflow'from this chamber aiding in the separation of the air into its constituents. In the form of the invention shown in F ig. 3 the tank 15 is in communication through the tube 15 with the distilling column adjacent the upper stage thereof so that nitrogen delivered through the pipe 14 will, as it overflows the tank 1'5, fall within the upper portion of said distilling column in a manner to meet the incoming vapors in the manner described in connection with the form of the invention shown in Fig. 1. The tank 15 and coil 16 are used for conditioning the air prior to its delivcry to the distilling column thus performing the function for which the refrigerator 4 and its appurtenances is designed in the v form of the invention shown in Fig. 1.

In the modification of the invention shown in Fig. 4, the distilling column 41, boiler 39. and vaporizer 40 are the same as in the pre ferred form of the invention. The arrangement of exchangersis also the same as that shown in Fig. 1, although these exchangers are not used to impartcold to the nitrogen passing to the condenser. In this form of the invention, the condensing chamber 42,

by means of which the liquid oxygen in the boiler and vaporizer is converted into a gas or vapor, is at the top of a distilling column into which the air. to be treated-is delivered through the pipe 37 containing thereinthe valve 37*. The contact of the air delivered through this pipe with the nitrogen upon the desired temperature and it will pass with some nitrogen all probability through the pipe 43 to a stage of the column 41. In the meanwhile, the nitrogen rising} to the top'of the column 38 will act upon the oxygen in the boiler and in the vaporizer ing into it are the tubes 48 pipes 48 with a drum 148.

the condenser chamber 59 and the condensed portion thereof will pass upwardly through the pipe 32 upon the upper stage ofj'the column 41. The efiect of the structure shown in Fig. 4 and its mode ofo'peration excepting as to the manner ofconditioning theair for delivery to the main distilling column is the same as that shown in Fig. 1.

denser for the nitrogen at 51. Centrally of;

said condenseris achamber 51 Discharg 10W head 48 and located in the boiler 45.

,The' head 48 is in communication through 1n turn is inv communication through the This drum is in communication through the pipes 148 with a drum 149 communicating through the pipe 150 with the distilling column-151.

- At 152 I have shown the nitrogen pipe for delivering the liquid nitrogen to the the pipes 48* with 'a second head 48 which carried by a holupper portion of a distilling column surmounting the'boiler 45 and at 153 I have shown an oxygen ofi'take pipe for Withdrawing oxygen from the chamber 154. corresponding with the chamber 26 in the form of the invention shown in Fig. 1. The tubes 49 and 50" lead from the condensing chamber 51 into the boiler 45 to the chamber 154 for thepurposeof securing a more effective ebullition of the liquid oxygen contained in said boiler and said chamber. The pipe 46 extends from the drum 148 to one of the stages of the distilling column 151 for the purpose of delivering the conditioned air to this column. In this form of'the invention the a'r to be treated is first distilled in the coluihn 151 the product passing through the pipe15O and the various heads and tubes communicating therewith, some nitrogen being delivered to. the condenser '51 and the remainder of the products being re-delivered to the column 151 through the pipe 46 from whence they pass to the distilling column surmounting the boiler 45 in the manner shown and described in connection with the form of the invention shown in Fig. 4 of the accompanying drawings.

In the modification shown in Fig. 6, the main multiple stage distilling column is shown at 60, the liquid nitrogen being deboiler 162 surrounded by a chamber 163, in

communication therewith through the duct 'livered to the upper part of this column a boiler 162 and chamber 163 respectively, thus facilitating the condensation of the,

tion thereof. Difierent portions of the bulb communication with said chamber,

mif'wahin theboiler 52 into-which oxygen. is discharged from the lowermost stage of the column '60 through the pipe 164.- Below the condensing chamber 59 is a distilling column 66 for the treatment of the air preliminary to its delivery to the distilling ocolumn 60, air being of said column 66, through the Within the condensing chamber 59 tition 166 open at the top so as is a parto be in and havat the bottom thereof a trough indicated at 167. Seated inthe trough 167 is the lower enlarged head of a conduit 168 opening into a drum 169. A plurality of tubes 170 extend from said drum anddischarge into the space Within said partition 166. A plurality of tubes'171- project from the space within .said partition 166 and from the condenser chamber 59 into the nitrogen passed through the'tubes 171 and the volatilization of the oxygen contained in said boiler and said chamber. .The air deliveredthrough the pipe 165 passes upwardly through the distllling column 66 and is brought to the desired temperature and par tially rectified. This air passes through the tube 100' and the pipe 168 to the drum 169 from whence it falls backwardlythrough the tubes/170 to withinthe compartment 166. Through this circulation, it is caused to give up a considerable'percentage of its heat to the oxygen within the boiler 162. The air, due to the lowering in its temperature, will accumulate within the partition 166 until it overflows the trough 167 and falls through the pipe 100 passing downwardly through the distilling column 66 until it reaches the bottom thereof. To

avoid such ebullition of this air while in the bottom of the column 66 as will unnecessarily agitate it, I surround the bottom of the column with the liquid accumulated in the bottom of the column 66 is delivered through the pipe 172 having in the length thereof an .expan-,

sion valve 54. To prevent the passage of frozen mist or .of solidified carbonic acid, to the lower portion of the column 66- I provide a decantation diaphragm 53. In

conjunction with the condenser 59, I provide'a sight gage for indicating the conditions within said condenser consisting of a bulb 56, afloat 57 and a cap. 58 surround-. mg the upper portion o'f'the bulb: 56, as p perfect a vacuum as is practicable being maintained between said cap and said bulb for the purpose of insulating the upper por- 56 are connected respectively with the upper and the lower portions ofthe chamber 59. 4

162 is a diaphragm which may delivered adjacent thelower portion pipe 165.

its constituents,

.tiple stage distilling column,

a jacket 55 into which and 8 illustrate an arrangement be applied to the upper portlon of the main distilling columns here- Figs. 7

of any tofore described. This device comprises a refrigerating coil 62, 63 and- 64 upon which a portion of the-nitrogen vapors beyond the upper stage of the column is adapted to condense in order to retard the flow of gas from said upper stages. This device also serves as a compensation throughout the apparatus through the reduction of the temperature of the nitrogen for the loss of heat thereby. In Fig. 7 this column is shown in a casing independent of the I column shown at 61, while .in Fig. 8 the coil is shown in the UPPBIIPOIHOII of this column.

In the forms of the invention shown in Figs. 7 and 8 the desired operative efiect is secured by expanding nitrogen in the coil 62, 63 being the inlet-extension of said coil "and 64 the outlet extension.

While I have shown- "-various constructions adapted for separating the air into limit the invention to thevarious constructions' shown. The essential characteristics of the apparatus employed are a main mulmeans for, bringing air to the temperature of its saturated vapors before introducing it to a stage intermediate the top and bottomfof said column, means for introducing liquid nitrogen adjacent the top of said column, a receptacle for liquid ox gen in communication with the bottom 0 said column and a condenser adjacent said last named means tically the same in each form of the invention shown. Having described the invention what I claim as new and desire to have protected .by Letters Patent is 2- w 1. An apparatus for separating air into its constituents embodying therein a multiple stage distilling column, means wherein air may be brought to the temperature of its saturated vapors,

saidmeans an'dsaid column, a boiler into which liquid oxygen is delivered from the lowermost stage of said column, means adapted to receive. an agent whereby the oxygen-in said boiler may be vaporized, means whereby oxygen in said boiler is withdrawn in gaseous form therefrom andmeans it is not my intention to.

the variations Y connections between- In each v deliveringliquid"nitrogen to the upper portion ofisaid column."

- 1ts constituents embodying therein a mul- ;2 -An -appara tus forseparating i i' b its constituents embodying therein a mul tiple stage distilling column, means wherein an may be brought to the temperature of its saturated vapors, connections between said means and said column, aboiler into which liquid oxygen is delivered from the lowermost stage of said column, a condenser in surface contact with said boiler, means adapted to deliver nitrogen to saidcon denser, whereby the oxygen in said boiler may be volatilized,. -means whereby oxygen in said boiler is withdrawn in gaseous form therefrom and means conveying liquid ni-. trogen from said. condenser to the upperv portionof said collinm.

3. An apparatus for separating air into its constituents embodying therein a multiple stage distilling column, means wherein air may be brought to the temperatureof its saturated vapors, connections between said means and said column, a boiler into which liquid oxygen is delivered from the lowermost stage of said column, means adapted to receive an agent whereby the oxygen in said boiler may be vaporized,

means whereby oxygen in said boiler is withdrawn in gaseous form therefrom, means delivering liquid nitrogen to the upper por- 8 tion of said column, and means whereby cold of compensation is delivered'to said column with the air.

4. An apparatus for separating air into tiple stage distilling column, means wherein air may be brought to the temperature of its saturated vapors v lncluding therein means for removing impurities from the air before delivering the air to said column,

ing liquid nitrogento the upper portion of' said column.

5. An apparatus for separatingair into its constituents embodying therein a multiple stage distilling column, means wherein air may be brought to the temperature of its saturated vapors, connections between said means and said column, a boiler into which liquidoxy en is delivered from the lowermost stage ,0 said column, a condenser insurface contact with said boilerand means -maintaining a continuous circulation of nitrogen from the upper part of said column in the form of gas through said condenser where it is liquefied and back to the upper part of sad column.

- '6. An. apparatus for separatingairinto its saturated vapors, connections between ,said means and said column, a boiler into which liquid oxygen ,lS delivered from the lowermost stage of said column, means adapted to receive an agent whereby the oxygen in said boiler may be vaporized, a vaporizer surrounding and in communicaa its constituents embodying therein a mul- "tiple stage distilling column, means wherein air may be brought to the temperature of tion with said boiler, an ofl'take leading from said vaporizer, and means delivering liquidnitrogen to the upper portion of said 7 column. v

7. An apparatus for separating air intoits constituents embodying therein a multiple stage distilling column, means wherein air may be brought to the temperature of its saturatedjvapors, connections between saidmeans and said column, a boiler into which liquid oxygen is delivered from the lower most stage of said column, means adapted togeceive an'agent whereby the oxygen in sai boiler may be vaporized, a vaporizer surrounding said boiler, a siphon tube connecting said boiler and said vaporizer, an

ofi'take leading fromsaid vaporizer, and means delivering liquid nitrogen to the upper portion of said column.

An apparatus for separating air into its constituents embodying therein, a multiple stage distilling column, means-wherein air may be brought to the temperature of its saturated vapors, connections between said means and said column, a heat exchanger, an

air pipe passing through said heat exchanger and' discharging into said first named means, a boiler into which liquid oxygen is delivered from the lowermost stage .of said column, a condenser, means withdrawing gaseous nitrogen from the top of said column, connections between said 7 means and said condenser, connections-between said condenser and the upper part of said column and means whereby oxygen in 1 said boiler is withdrawn in gaseous form. a

9. An apparatus for separating air into its constituents embodying therein -a mul tiplestage distilling column, means wherein air may be brought to the temperature of its saturated vapors, connections between said means andsaid column,a boiler into which liquid oxygen is delivered from the lower most stage of said column, a vaporizer surrounding and in communication with said boiler, a condenser in surface contact with said boiler and said vaporizer, a heat .exchanger, an oflitake leadingfrom. said vaporizer and discharging into said heat ex-' changer, and means withdrawing gaseous} nitrogen from the upper portion of said .cQlumn, Passing it through Said, heat changer, delivering it t said con-denser,

tiple stage distilling column,

intermediate the uppermost and withdrawing it from said condenser and delivering it to the upper I portion of said column. i v

10. An apparatus for separating air into its constituents embodying therein a mula refrigerating chamber, a connection between said refrigerating chamber and a stage of said column lowermost stages thereof, means whereby air under pressure may be delivered to and expanded in said chamber,tubes in said chamber, a boiler adapted to receive liquid oxygen from the lowermost stage of said column, a vaporizer about said boiler, a condenser in surface .contact with said boiler and said vaporizer, an ofi'take-pipe whereby oxygen may be withdrawn from said vaporizer, a nitrogen ofitake pipe communicating with the upper portion of said column, a plurality of heat exchangers communicating respectively with said oxygen ofitake pipe and said nitrogen ofitake pipe, said means for delivering air under pressure to said chamber passing through one of said heat exchangers, means withdrawing nitrogen from said column through said ofltake pipe and one of said heat exchangers, a pipe connection between said last named means and said tubes, passing through both of said heat exchangers, a pipe connection between said tubes and said-condenser and a pipe connection between said upper portion of said column whereby there is a continuous circulation of nitrogen, leaving the upper portion of said column in a gaseous form and entering the upper portion of said column in a liquid form.

condenser and the In testimony whereof I afiix my signature,

in presence of two witnesses.

MAURICE HAZARD-FLAMAND. Witnesses:

PAUL COULOMB, H. C. COKE. 

